反应详情

温度

95 °C

In a 100 ml round bottom flask equipped with magnetically stirring, thermometer, reflux condenser and addition funnel, 6,11-dihydro-5H-dibenz[b,e]azepine (1.0 g, 5,1 mmol, prepared in a similar way as described in Coll. Czech. Chem. Commun., 23, 1958, 1330) was dissolved in dry toluene (25 ml). 3-Chloropropionyl chloride (0.78 g, 6,1 mmol) was added slowly. When addition was complete, the reaction mixture was heated at 95° C. for 30 minutes and then allowed to cool to room temperature. With stirring, 0.2N sodium hydroxide (2.5 ml) was added. More toluene (50 ml) was added and the phases were separated. The organic phase was washed with 0.2N sodium hydroxide (10 ml) until pH>10, and then with water (3×10 ml) and brine (10 ml). After drying (MgSO4), the solvent was evaporated in vacuo affording 3-chloro-1-(6,11-dihydro-5H-dibenz[b,e]azepin-5-yl)-1 -propanone as an oil which was obtained in quantitative yield and used for further reactions without purification.

1. customIn a 100 ml round bottom flask equipped
2. temperaturethermometer, reflux
3. additioncondenser and addition funnel
4. additionWhen addition
5. temperatureto cool to room temperature
6. stirringWith stirring
7. customthe phases were separated
8. washThe organic phase was washed with 0.2N sodium hydroxide (10 ml) until pH>10
9. dry with materialAfter drying (MgSO4)
10. customthe solvent was evaporated in vacuo